CN1654616A - combined extraction method for rosemary essential oil and rosemary antioxidant - Google Patents
combined extraction method for rosemary essential oil and rosemary antioxidant Download PDFInfo
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- CN1654616A CN1654616A CNA2005100382153A CN200510038215A CN1654616A CN 1654616 A CN1654616 A CN 1654616A CN A2005100382153 A CNA2005100382153 A CN A2005100382153A CN 200510038215 A CN200510038215 A CN 200510038215A CN 1654616 A CN1654616 A CN 1654616A
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Abstract
The comprehensive process of extracting refined rosemary oil and rosemary antioxidant includes the following steps: circularly extracting rosemary leaf directly with polar organic solvent in 3-20 times rosemary leaf at 20-100 deg.c for 0.08-6 hr to obtain refined rosemary oil and rosemary antioxidant dissolved in the polar organic solvent; circularly extracting the mixture of refined rosemary oil and rosemary antioxidant directly with non-polar organic solvent or weak polar organic solvent in 3-200 times the mixture at 20-100 deg.c for 0.08-6 hr and cooling to 5-30 deg.c to obtain refined rosemary oil dissolved in the non-polar organic solvent or weak polar organic solvent and rosemary antioxidant deposit; filtering to obtain rosemary antioxidant; and distilling the extracted liquid at 20-100 deg.c to eliminate solvent and obtain refined rosemary oil. The said process has short extraction period, high efficiency and low cost.
Description
Technical field
The present invention relates to the extracting method of a kind of rosemary ethereal oil and rosemary antioxidant, relate in particular to and a kind ofly extract through polar organic solvent, nonpolar or weakly polar organic solvent or the circulation of its mixed solvent by the Rosmarinus officinalis cured leaf, auxiliaryly in case of necessity handle, synchronously or successively obtain the combined extraction method of rosemary ethereal oil and rosemary antioxidant with intensified by ultrasonic wave.
Background technology
The extracting method of rosemary ethereal oil mainly is to use the traditional water vapor distillation method, and use CO is also arranged in the recent period
2Supercritical extraction.The extracting method of rosemary antioxidant comprises: " food oils extraction method ", " organic solvent extraction method ", " CO
2Supercritical extraction ", " potass extraction method " and " superheated water extraction method " etc." food oils extraction method " is the Rosmarinus officinalis leaf to be pulverized the back directly use the food oils lixiviate under room temperature or heated condition, but filter and remove residue speed is slow, and have denseer rosemary ethereal oil peculiar smell in the oil, difficulty eliminates: " organic solvent extraction method " is that a class is used early, and economic and practical extracting method, according to the difference of using solvent species, its extracting method and step also have nothing in common with each other; " CO
2Supercritical extraction " extraction effect is good, quality product is high; and but small, apparatus expensive, high top pressure operation, running cost are higher; this method is extracted favourable to volatile essential oil; nonvolatile rosemary antioxidant is extracted also need add a small amount of organic solvent and make entrainment agent or cosolvent; extract yield or selectivity to improve, and have in fact also lost not advantage with an organic solvent; " potass extraction method " has considerable influence to some activeconstituents in the raw material, and the product appearance that obtains is poor, uses yield low separately, and needs the strict pH scope that control extracting solution well; " superheated water extraction method " just has the preliminary study report, and this method does not also have moulding, and extraction element is special, and scale is very little, also do not possess application and development and is worth.
In existing " organic solvent extraction method " close with the present invention, comprise the residual leaf that steamed with extraction using alcohol Rosmarinus officinalis raw material or water vapor, desolvating obtains paste, cooks off steps such as the water solubles again through boiling water, can obtain the powdery rosemary antioxidant; Adopt ethanol-hexane mixed solvent extraction of 2～95%, also can obtain rosemary antioxidant through thin up; The acetone room temperature is extracted, and can remove oxide additive matter such as chlorophyll, obtains complete oil-soluble rosemary antioxidant; Under room temperature and nitrogen, through the hexane preimpregnation, extraction using alcohol residue and decolouring again can obtain the powdery rosemary antioxidant; Use the mixed solvent of Tetrafluoroethane and acetone to extract Rosmarinus officinalis, can obtain the oily liquids rosemary antioxidant, but extraction yield is lower, Tetrafluoroethane valency height is difficult to obtain, and under the room temperature gaseous state, thus equipment requirements harsh (high pressure), solvent recuperation conditional request height.On the whole, the said extracted method is the extracting method of independently setting up at the single product of rosemary antioxidant, extraction is based on single lixiviate at intermittence means, do not have more economical the extracting synchronously or successively of rosemary ethereal oil and rosemary antioxidant of reasonably taking all factors into consideration, do not see the patented method of using intensified by ultrasonic wave rosemary ethereal oil and rosemary antioxidant leaching process simultaneously yet.
Summary of the invention
The invention provides that a kind of cost is low, extraction rate is fast, extraction efficiency is high, the dissolvent residual less contamination is little and reclaim the combined extraction method of rosemary ethereal oil and rosemary antioxidant easily.
The invention provides following technical scheme:
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant, it is characterized in that extracting rosemary leave material 0.08～6h 20～100 ℃ of direct down circulations with the polar organic solvent of 3～20 times of weight that are equivalent to the rosemary leave material, acquisition is dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant, nonpolar or weakly polar organic solvent with 3～200 times of weight of mixture that are equivalent to rosemary ethereal oil and rosemary antioxidant extracts rosemary ethereal oil and rosemary antioxidant 0.08～6h and is cooled to 5～30 ℃ 20～100 ℃ of direct down circulations, acquisition is dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and the rosemary antioxidant of precipitation shape, filter, obtain the throw out rosemary antioxidant, extracting solution boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
Wherein directly extract with polar organic solvent and obtain to be dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant, and separate, method is as follows:
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant comprises following two steps:
The first step: use the polar organic solvent that is equivalent to 3～20 times of weight of rosemary leave material directly to circulate down at 20～100 ℃ and extract rosemary leave material 0.08～6h, extracting solution is boiled off solvent under 20～100 ℃, obtain the mixture of rosemary ethereal oil and rosemary antioxidant;
Second step: at 20～100 ℃ of nonpolar or weakly polar organic solvents of using 3～20 times of weight of mixture that are equivalent to above-mentioned rosemary ethereal oil and rosemary antioxidant down, directly the mixture 0.5～6h of above-mentioned rosemary ethereal oil and rosemary antioxidant is extracted in circulation, be cooled to 5～30 ℃, filter, the solid that obtains is the rosemary antioxidant product, filtrate boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
In addition, directly extract with the mixture of nonpolar or weakly polar organic solvent and polar organic solvent and to obtain to be dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and the rosemary antioxidant of precipitation shape, and separate, method is as follows:
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant, earlier under 20～100 ℃, mixed organic solvents with polar organic solvent and nonpolar or weakly polar organic solvent, directly rosemary leave material 0.08～6h is extracted in circulation, the gross weight of the mixed organic solvents of wherein nonpolar or weakly polar organic solvent and polar organic solvent is 3～20 times of rosemary leave material weight, it is 0.1～20% that polar organic solvent weight accounts for per-cent nonpolar or weakly polar organic solvent and polar organic solvent gross weight, postcooling to 5～30 ℃ are extracted in circulation, obtain containing the extracting solution of light insoluble solids rosemary antioxidant, filter, the solid that obtains is the rosemary antioxidant product, and filtrate boils off solvent and obtains the rosemary ethereal oil product under 20～100 ℃.
The present invention also can expect to adopt synchronously in the circulation leaching process ultrasonic wave to strengthen the effect of extraction, ultrasonic frequency 20～40KHz, ultrasonic power 100～2000W, circulation extraction time 5～60min rosemary leave.
Principle of the present invention:
The circulation extracting apparatus that the present invention relates to, it can be Soxhlet extractor type circulation extracting apparatus, it also can be simple power transmission circulation extracting apparatus, they all are made up of extractor and receptor two big major portions, be aided with reflux (being the Soxhlet extractor type) simultaneously, or power transmission (being the power transmission circular form), heating and cooling unit, realize the pump circulation of organic solvent between extractor and receptor, reach the purpose that the Rosmarinus officinalis leaf is repeatedly circulated and extracts and improve extract yield.
The working process and the flow process of Soxhlet extractor type circulation extracting apparatus:
(1) in Soxhlet extractor type circulation extracting apparatus extractor and junction, overflow siphon pipe bottom a little cotton of pad, the Rosmarinus officinalis leaf is packed in the extractor, leaf is packed into and is not highly surpassed overflow siphon pipe apical position, the extractor bottom is connected to receptor, extractor top is connected to condenser, and receptor has heating unit outward and has the evaporation conduit to communicate with the condenser on extractor top;
(2) will extract with organic solvent and slowly be joined in the extractor that fills the Rosmarinus officinalis leaf by extractor top, and make leaf be complete soaking state, Fu Yu solvent slowly flows in the receptor of bottom with the overflow siphon pipe simultaneously;
(3) open the reflux unit, solvent in the receptor of bottom constantly is subjected to thermal evaporation, enter the condenser on extractor top through the evaporation conduit, and by rapid condensation, inflow fills in the extractor of Rosmarinus officinalis leaf, the Rosmarinus officinalis leaf is implemented lixiviate, in the extractor lixiviate organic solvent liquid level of rosemary ethereal oil and rosemary antioxidant raise gradually, when reaching overflow siphon pipe apical position, because syphonic effect flow in the receptor of bottom the organic solvent that contains rosemary ethereal oil and rosemary antioxidant fast by siphon pipe;
(4) organic solvent that contains rosemary ethereal oil and rosemary antioxidant bottom in the receptor is subjected to thermal evaporation continuously, form the organic solvent steam that does not contain rosemary ethereal oil substantially and do not contain rosemary antioxidant fully, enter condenser condenses, entering extractor again extracts, go round and begin again, realize " evaporation-condensation-extraction " circulation leaching process, and rosemary antioxidant does not participate in the solvent cycle process of this " evaporation-condensation-extraction ", progressively be accumulated in the receptor, rosemary ethereal oil may have the part low boiling component and participate in this working cycle, but main component also is accumulated in the receptor;
(5) the leaf residue that has fully been extracted rosemary ethereal oil and rosemary antioxidant is still stayed in the extractor, behind the organic solvent that drop goes to adsorb, residue poured out discards.
The working process and the flow process of power transmission circular form extraction element:
(1) in the extractor bottom of power transmission circular form extraction element filter screen is housed, and link to each other with the receptor of extractor bottom, the organic solvent spray header is equipped with at the extractor top, receptor has cooling unit and power-driven pump cycling element outward, and circulating line is communicated with extractor top spray head by the pipeline of susceptor through power-driven pump and band heating unit.The Rosmarinus officinalis leaf evenly is encased on the filter screen of extractor;
(2) will extract with organic solvent and slowly be joined in the extractor that fills the Rosmarinus officinalis leaf by extractor top spray header, and make leaf be half and soak or soaking state fully, Fu Yu solvent is bottom screen cloth slowly flows in the receptor simultaneously;
(3) turn on the power pump and the heating cooling unit, solvent in the receptor of bottom is constantly entered in the extractor by receptor, water back and spray header by power-driven pump, and to Rosmarinus officinalis leaf enforcement lixiviate, in the extractor lixiviate organic solvent of rosemary ethereal oil and rosemary antioxidant through the bottom screen filtration, enter into the bottom receptor of band cooling unit again;
(4) contain the organic solvent of rosemary ethereal oil and rosemary antioxidant continuously by power-driven pump transmission, spray and lixiviate in the receptor of bottom, rosemary ethereal oil and rosemary antioxidant concentration improve gradually in the organic solvent, essential oil and oxidation preventive content reduce gradually along with the increase of stripping quantity in the extractor Rosmarinus officinalis leaf, thereby have realized the circulation leaching process.In this circulation leaching process, rosemary ethereal oil participates in this working cycle all the time, rosemary antioxidant is then distinguished to some extent according to the difference of extracting solvent species, under the polar solvent state, rosemary antioxidant participates in this working cycle all the time, and under with the non-polar solvent state that contains the segment polarity solvent, rosemary antioxidant is because of extractor and susceptor upper and lower temperature difference reason, saturated gradually separating out in receptor, and progressively be accumulated in the receptor;
(5) the leaf residue that has fully been extracted rosemary ethereal oil and rosemary antioxidant is still stayed in the extractor, behind the organic solvent that drop goes to adsorb, residue poured out discards.
Directly extract and obtain to be dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant with polar organic solvent, and separate, in this technical scheme: the principle that the first step utilizes rosemary ethereal oil and rosemary antioxidant can be dissolved in organic polar solvent extracts them, and the principle that second step utilized rosemary antioxidant to be insoluble to non-polar solvent is separated rosemary antioxidant and rosemary ethereal oil by extracting in the mixture.Rosemary ethereal oil is with α-Pai Xi, 1, small molecule hydrocarbon compounds nonpolar or weakly polar organic solvent such as 8-cineole, amphene, beta-pinene are the mixture of main body, both can be dissolved by organic polar solvent, again can be by nonpolar or low-pole organic polar solvent dissolving; Rosemary antioxidant then by Salvin, carnosol, rosmarinic acid, Rosmarinus officinalis phenol, and other small molecules phenolic acid and the stronger compound of flavones isopolarity form, these compositions solvability in polar organic solvent is good, and is poorly soluble in nonpolar or weakly polar organic solvent.With macromolecular compounds such as Mierocrystalline cellulose, hemicellulose and xylogen is the rosemary leave residue of main body composition, and solvability is all very poor in polar organic solvent, nonpolar or weakly polar organic solvent.Therefore, rosemary ethereal oil and rosemary antioxidant can be obtained by extraction separation respectively through two step circulation leaching process.
Mixture with nonpolar or weakly polar organic solvent and polar organic solvent extracts the rosemary antioxidant that obtains to be dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and precipitate shape, and separate, this scheme utilization contains the sherwood oil mixed solution of segment polarity solvent to rosemary ethereal oil and rosemary antioxidant, the difference of solubility property under differing temps and CONCENTRATION STATE, realize that rosemary ethereal oil both separated with Rosmarinus officinalis leaf residue simultaneously with rosemary antioxidant, self separates with solid-state and solution state respectively again.At first, the sherwood oil mixed solution that contains the segment polarity solvent is to being that the rosemary leave residue of main body composition is insoluble substantially with macromolecular compounds such as Mierocrystalline cellulose, hemicellulose and xylogen, so Rosmarinus officinalis leaf residue just can not enter the bottom receptor; Secondly, the sherwood oil mixed solution that contains the segment polarity solvent is the rosemary ethereal oil of main body composition to the small molecule hydrocarbon compounds with low-pole, is all to have good solvability under comparatively high temps or lesser temps, stays in the solvent phase all the time after being extracted; Moreover, the sherwood oil mixed solution that contains the segment polarity solvent has certain dissolubility to rosemary antioxidant under comparatively high temps (low concentration), solvability is just poor down and at lesser temps (higher concentration), in working cycle repeatedly, constantly stripping from extractor of rosemary antioxidant, enter the bottom and will constantly from mixed solvent, separate out behind the susceptor, realize and contain separating of essential oil solvent phase.
The present invention obtains following technique effect:
(1) be extracted as the master with solvent cycle, the present invention can separate with nonpolar or weak polar solvent then with polar organic solvent with rosemary ethereal oil and rosemary antioxidant extraction and dissolving; Also can directly extract rosemary ethereal oil and rosemary antioxidant simultaneously, and simultaneously the rosemary ethereal oil and the rosemary antioxidant of precipitation shape be separated with the mixed solution of polar organic solvent and non-polar organic solvent.These two kinds of methods can realize extracting synchronously or successively of rosemary ethereal oil and rosemary antioxidant, and extracting cycle is short, efficient is high, cost is low;
(2) use the conventional organic solvent that is easy to get, cheap, it is convenient, residual few to reclaim, and pollutes little;
(3) the present invention is aided with intensified by ultrasonic wave extraction processing in rosemary leave material circulation leaching process, making intensified by ultrasonic wave extract processing combines with organic solvent circulation extract phase, utilize the CF cavitation effect of ultrasonic waves, make organic solvent under demulcent condition more (extract temperature low and extraction time is short), rapid osmotic is in the cell walls of Rosmarinus officinalis leaf, rosemary ethereal oil and rosemary antioxidant are dissolved fully apace to be distributed in the organic solvent, realize efficient rapid extraction process, ordinary cycle is extracted among the present invention needs 2～6h usually, and after being aided with intensified by ultrasonic wave extraction processing, extraction time shortens to 5～60min, thereby more help keeping the effective constituent of rosemary ethereal oil and rosemary antioxidant, guarantee the stay in grade of rosemary ethereal oil and rosemary antioxidant.Intensified by ultrasonic wave extracts easy to operate, be beneficial to industrial applications, and the running cost increase seldom.
(4) the present invention has realized separating of effective constituent and residue in the Rosmarinus officinalis leaf in lesser temps and short period, also in lesser temps and short period, realize separating of rosemary ethereal oil and rosemary antioxidant, energy consumption is low, need not use special high-tension apparatus, the equipment less investment, product is more difficult to change in the course of processing (when temperature is too high, the volatile loss of essential oil, rosemary antioxidant can be partly rotten).
(5) the rosemary antioxidant crude product can not contained chlorophyllous light rosemary antioxidant through the gac processing of decolouring in aqueous ethanolic solution.
Embodiment
Embodiment 1
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant, it is characterized in that extracting rosemary leave material 0.08～6h 20～100 ℃ of direct down circulations with the polar organic solvent of 3～20 times of weight that are equivalent to the rosemary leave material, acquisition is dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant, nonpolar or weakly polar organic solvent with 3～200 times of weight of mixture that are equivalent to rosemary ethereal oil and rosemary antioxidant extracts rosemary ethereal oil and rosemary antioxidant 0.08～6h and is cooled to 5～30 ℃ 20～100 ℃ of direct down circulations, acquisition is dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and the rosemary antioxidant of precipitation shape, filter, obtain the throw out rosemary antioxidant, extracting solution boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
In the present embodiment, can directly extract with polar organic solvent and obtain to be dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant, both be separated again, detailed process can be with reference to embodiment 2; Also available mixture nonpolar or weakly polar organic solvent and polar organic solvent directly extracts and obtains to be dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and the rosemary antioxidant of precipitation shape, and separates, and detailed process can be with reference to embodiment 3,
Wherein, raw material Rosmarinus officinalis cured leaf both can be the cured leaf of growth and maturity, it also can be the bright leaf of nature air dried, moisture content all≤10%, the Rosmarinus officinalis cured leaf can be ground into powder, also can be without pulverization process, polar organic solvent can for alcohols (as methyl alcohol, ethanol, propyl alcohol, butanols equal solvent, or its aqueous mixture), ketone (acetone, methylethylketone, pimelinketone equal solvent), ester class (methyl acetate, ethyl acetate, butylacetate equal solvent) etc., circulation extraction equipment can adopt the circulation of reflux formula to extract (as Soxhlet extractor).Also can adopt power transmission circulating (as the pump power circulation); Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 times, 8.3 times, 9.4 doubly, 10.5 times, 11.8 times, 12.5 times, 13.5 times, 14 times, 15.5 times, 16.5 times, 17.5 times, 19.2 doubly, can be 0.1h, 0.2h, 0.3h cycling time, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, and 60 ℃, 75 ℃; Extract and comprise alkane (sherwood oil of normal hexane, hexanaphthene, different boiling ranges etc.), alkane substitute (1 with nonpolar or weakly polar organic solvent, 1-ethylene dichloride, 1,2-ethylene dichloride, methylene dichloride, chloroform etc.), aromatic hydrocarbons (benzene, toluene etc.), ethers (ether, methyl ethyl ether etc.) etc.; Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of nonpolar or weakly polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 times, 8.3 times, 9.4 doubly, 10.5 times, 11.8 times, 12.5 times, 13.5 times, 14 times, 15.5 times, 16.5 times, 17.5 times, 19.2 times, 40 times, 70 times, 150 times, 185 times, can be 0.1h cycling time, 0.2h, 0.3h, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, and 60 ℃, 75 ℃.
Embodiment 2
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant comprises following two steps:
The first step: the rosemary leave material is mixed in circulation extraction equipment with the polar organic solvent that is equivalent to 3～20 times of weight of rosemary leave material, at 20～100 ℃ of extraction 0.08～6h that directly circulate down, the rosemary leave residue is stayed in the extractor, extracting solution in the receptor of bottom is boiled off solvent under 20～100 ℃, obtain the mixture of rosemary ethereal oil and rosemary antioxidant;
Wherein, raw material Rosmarinus officinalis cured leaf both can be the cured leaf of growth and maturity, it also can be the bright leaf of nature air dried, moisture content all≤10%, the Rosmarinus officinalis cured leaf can be ground into powder, also can be without pulverization process, polar organic solvent can for alcohols (as methyl alcohol, ethanol, propyl alcohol, butanols equal solvent, or its aqueous mixture), ketone (acetone, methylethylketone, pimelinketone equal solvent), ester class (methyl acetate, ethyl acetate, butylacetate equal solvent) etc., circulation extraction equipment can adopt the circulation of reflux formula to extract (as Soxhlet extractor).Also can adopt power transmission circulating (as the pump power circulation); Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 times, 8.3 times, 9.4 doubly, 10.5 times, 11.8 times, 12.5 times, 13.5 times, 14 times, 15.5 times, 16.5 times, 17.5 times, 19.2 doubly, can be 0.1h, 0.2h, 0.3h cycling time, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, and 60 ℃, 75 ℃;
Second step: the mixture of above-mentioned rosemary ethereal oil and rosemary antioxidant is mixed in circulation extraction equipment with the nonpolar or weakly polar organic solvent that is equivalent to 3～20 times of weight of mixture, at 20～100 ℃ of extraction 0.5～6h that directly circulate down, cooling, filter, the solid that obtains is the rosemary antioxidant product, extracting solution boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
Wherein, extract and comprise alkane (sherwood oil of normal hexane, hexanaphthene, different boiling ranges etc.), alkane substitute (1 with nonpolar or weakly polar organic solvent, 1-ethylene dichloride, 1,2-ethylene dichloride, methylene dichloride, chloroform etc.), aromatic hydrocarbons (benzene, toluene etc.), ethers (ether, methyl ethyl ether etc.) etc.; Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of nonpolar or weakly polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 times, 8.3 times, 9.4 doubly, 10.5 times, 11.8 times, 12.5 times, 13.5 times, 14 times, 15.5 times, 16.5 times, 17.5 times, 19.2 doubly, can be 0.1h, 0.2h, 0.3h cycling time, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, and 60 ℃, 75 ℃.
Embodiment 3
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant, earlier under 20～100 ℃, mixed organic solvents with polar organic solvent and nonpolar or weakly polar organic solvent, directly rosemary leave material 0.08～6h is extracted in circulation, the gross weight of the mixed organic solvents of wherein nonpolar or weakly polar organic solvent and polar organic solvent is 3～20 times of rosemary leave material weight, it is 0.1～20% that the weight of polar organic solvent accounts for per-cent nonpolar or weakly polar organic solvent and polar organic solvent gross weight, postcooling to 5～30 ℃ are extracted in circulation, obtain containing the extracting solution of light insoluble solids rosemary antioxidant, filter, the solid that obtains is the rosemary antioxidant product, filtrate boils off solvent and obtains the rosemary ethereal oil product under 20～100 ℃
Wherein, raw material Rosmarinus officinalis cured leaf both can be the cured leaf of growth and maturity, also can be the bright leaf of nature air dried, moisture content all≤10%, the Rosmarinus officinalis cured leaf can be ground into powder, also can be without pulverization process, circulation extraction equipment can adopt the circulation of reflux formula to extract (as Soxhlet extractor), also can adopt power transmission circulating (as the pump power circulation), polar solvent and nonpolar or weakly polar organic solvent mixed solution, comprise sherwood oil, sherwood oil-ethanol, sherwood oil-alcohol-water, petroleum ether-ethyl acetate, sherwood oil-ethanol-ethyl acetate, petroleum ether-ethyl acetate-water, a kind of in the mixing solutionss such as sherwood oil-water, temperature is extracted in circulation can be 25 ℃, 30 ℃, 35 ℃, 60 ℃, 75 ℃, the gross weight of nonpolar or weakly polar organic solvent and polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 doubly, 8.3 times, 9.4 times, 10.5 doubly, 11.8 times, 12.5 times, 13.5 doubly, 14 times, 15.5 times, 16.5 doubly, 17.5 times, 19.2 times, the per-cent that polar organic solvent accounts for nonpolar or weakly polar organic solvent and polar organic solvent gross weight can be 0.3%, 0.8%, 1.0%, 2.3%, 3.2%, 5.8%, 8.5%, 9.9%, 12.6%, 13.5%, 15.7%, 18.9%, can be 0.1h cycling time, 0.2h, 0.3h, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, 60 ℃, 75 ℃.
Embodiment 4
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant comprises following two steps:
The first step: the rosemary leave material is mixed in circulation extraction equipment with the polar organic solvent of 3～20 times of weight, at 20～100 ℃ of extraction 5～60min that directly circulate down, and at this leaching process of circulation extraction time inter-sync loading intensified by ultrasonic wave, ultrasonic frequency 20～40KHz, ultrasonic power 100～2000W, can adopt the bath type ultrasonic generator, also can adopt the probe type ultrasonic wave generating device, cooling then, the rosemary leave residue is stayed in the extractor, extracting solution in the receptor of bottom is boiled off solvent under 20～100 ℃, obtain the mixture of rosemary ethereal oil and rosemary antioxidant;
Wherein, raw material Rosmarinus officinalis cured leaf both can be the cured leaf of growth and maturity, it also can be the bright leaf of nature air dried, moisture content all≤10%, the Rosmarinus officinalis cured leaf can be ground into powder, also can be without pulverization process, polar organic solvent can for alcohols (as methyl alcohol, ethanol, propyl alcohol, butanols equal solvent, or its aqueous mixture), ketone (acetone, methylethylketone, pimelinketone equal solvent), ester class (methyl acetate, ethyl acetate, butylacetate equal solvent) etc., circulation extraction equipment can adopt the circulation of reflux formula to extract (as Soxhlet extractor).Also can adopt power transmission circulating (as the pump power circulation); Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 doubly, 8.3 times, 9.4 times, 10.5 times, 11.8 doubly, 12.5 times, 13.5 times, 14 times, 15.5 doubly, 16.5 times, 17.5 times, 19.2 times, hyperacoustic power can be 300W, 700W, 1000W, 1500W, can be 0.1h, 0.2h, 0.25h, 0.3h cycling time, 0.32h, 0.42h, 0.5h, 0.66h, 0.8h, 0.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, 60 ℃, 75 ℃;
Second step: the mixture of above-mentioned rosemary ethereal oil and rosemary antioxidant is mixed in circulation extraction equipment with 3～20 times (weight ratio) nonpolar (or low-pole) solvent, at 20～100 ℃ of extraction 0.5～6h that directly circulate down, cooling, filter, the solid part that obtains is a rosemary antioxidant, extracting solution boils off solvent under 20～100 ℃, obtain rosemary ethereal oil.
Wherein, extract and comprise alkane (sherwood oil of normal hexane, hexanaphthene, different boiling ranges etc.), alkane substitute (1 with nonpolar or weakly polar organic solvent, 1-ethylene dichloride, 1,2-ethylene dichloride, methylene dichloride, chloroform etc.), aromatic hydrocarbons (benzene, toluene etc.), ethers (ether, methyl ethyl ether etc.) etc.; Temperature is extracted in circulation can be 25 ℃, 30 ℃, and 35 ℃, 60 ℃, 75 ℃, the weight of nonpolar or weakly polar organic solvent can be for being equivalent to 4 times of rosemary leave material, and 5.2 times, 6.5 times, 7.5 times, 8.3 times, 9.4 doubly, 10.5 times, 11.8 times, 12.5 times, 13.5 times, 14 times, 15.5 times, 16.5 times, 17.5 times, 19.2 doubly, can be 0.1h, 0.2h, 0.3h cycling time, 0.42h, 0.5h, 0.8h, 1h, 2h, 3h, 3.1h, 3.3h, 3.1h, 3.5h, 3.8h, 3.9h, 4h, 4.5h, 5.3h, 5.9h, the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, and 60 ℃, 75 ℃.
Embodiment 5
The combined extraction method of a kind of rosemary ethereal oil and rosemary antioxidant, at first rosemary leave is expected, polar solvent and non-polar solvent mix in circulation extraction equipment, wherein the gross weight of non-polar solvent or weakly polar organic solvent and polar organic solvent is 3～20 times that rosemary leave is expected weight, it is 0.1～20% that polar organic solvent accounts for per-cent nonpolar or weakly polar organic solvent and polar organic solvent gross weight, then under 20～100 ℃, directly 5～60min is extracted in circulation, directly adopting intensified by ultrasonic wave to extract synchronously in the circulation leaching process, ultrasonic frequency 20～40KHz, ultrasonic power 100～2000W, can adopt the bath type ultrasonic generator, also can adopt the probe type ultrasonic wave generating device, the rosemary leave residue is stayed in the extractor, cooling, from the receptor of bottom, obtain containing the extracting solution of a large amount of light insoluble solids, filter, can directly obtain light rosemary antioxidant solid, filtrate boils off solvent and obtains rosemary ethereal oil under 20～100 ℃.
Wherein, raw material Rosmarinus officinalis cured leaf both can be the cured leaf of growth and maturity, also can be the bright leaf of nature air dried, moisture content all≤10%, the Rosmarinus officinalis cured leaf can be ground into powder, also can be without pulverization process, and circulation extraction equipment can adopt the circulation of reflux formula to extract (as Soxhlet extractor), also can adopt power transmission circulating (as the pump power circulation), the mixed solution of polar solvent and nonpolar or weakly polar organic solvent can comprise sherwood oil, sherwood oil-ethanol, sherwood oil-alcohol-water, petroleum ether-ethyl acetate, sherwood oil-ethanol-ethyl acetate, petroleum ether-ethyl acetate-water, a kind of in sherwood oil-water, temperature is extracted in circulation can be 25 ℃, 30 ℃, 35 ℃, 60 ℃, 75 ℃, the gross weight of nonpolar or weakly polar organic solvent and polar organic solvent can be for being equivalent to 4 times of rosemary leave material, 5.2 doubly, 6.5 doubly, 7.5 times, 8.3 times, 9.4 doubly, 10.5 doubly, 11.8 times, 12.5 times, 13.5 doubly, 14 times, 15.5 times, 16.5 times, 17.5 doubly, 19.2 doubly, the polar organic solvent per-cent that accounts for nonpolar or weakly polar organic solvent and polar organic solvent gross weight can be 0.3%, 0.8%, 1.0%, 2.3%, 3.2%, 5.8%, 8.5%, 9.9%, 12.6%, 13.5%, 15.7%, 18.9%, can be 0.1h, 0.2h cycling time, 0.3h, 0.42h, 0.5h, 0.65h, 0.8h, 0.9h the temperature of evaporation organic solvent can be 25 ℃, 30 ℃, 60 ℃, 75 ℃.
Embodiment 6
The 10.0g Rosmarinus officinalis leaf of packing in the circulation extractor is pulverized material (particle is less than 2mm), put into 50～150mL polar solvent (as acetone, methyl alcohol, ethanol, 95% ethanol, ethyl acetate or 1: 1 ethanol-ethyl acetate mixed solvent) in the susceptor of bottom, 3～4h is extracted in circulation, cooling; With the extracting solution normal pressure or the underpressure distillation of polar solvent, obtain brown or blackish green medicinal extract (being general extractive); Medicinal extract is reinstalled in the extractor, and nonpolar or weak polar solvent carries out extract at low temperature with 50mL, and extracting solution obtains dark half liquid half material admittedly through underpressure distillation again, obtains colourless or light yellow rosemary ethereal oil through steam distillation again; General extractive obtains rosemary antioxidant crude product (the results are shown in Table 1) after nonpolar or weak polar solvent extracting.
Rosemary ethereal oil and rosemary antioxidant comprehensively extract the result under the table 1 opposed polarity solvent condition
No polar solvent general extractive (g) essential oil (g) rosemary antioxidant crude product (g)
1 acetone 1.65 0.26 0.96
2 methyl alcohol 2.48 0.16 1.78
3 ethanol 1.83 0.11 1.09
4 95% ethanol 2.48 0.13 1.43
5 ethyl acetate 1.80 0.28 0.95
6 ethanol-ethyl acetate (1: 1, v/v) 1.88 0.21 0.98
Embodiment 7
The 10.0g Rosmarinus officinalis leaf of packing in the circulation extractor is pulverized material (particle is less than 2mm), puts into 50～150mL polar solvent (as 95% ethanol) in the susceptor of bottom, and 1～6h is extracted in circulation, cooling; With the extracting solution normal pressure or the underpressure distillation of polar solvent, obtain brown or blackish green medicinal extract (being general extractive); Medicinal extract is reinstalled in the extractor, and nonpolar or weak polar solvent carries out extract at low temperature with 50mL, and extracting solution obtains dark half liquid half material admittedly through underpressure distillation again, obtains colourless or light yellow rosemary ethereal oil through steam distillation again; The rosemary antioxidant crude product that general extractive obtains after nonpolar or weak polar solvent extracting (the results are shown in Table 2).
Rosemary ethereal oil and rosemary antioxidant comprehensively extract the result under the different circulation of table 2 extraction times
No extraction time (h) general extractive (g) essential oil (g) rosemary antioxidant crude product (g)
7????????1???????????1.81????????0.11???????????1.26
8????????2???????????1.97????????0.13???????????1.39
9????????3???????????2.09????????0.14???????????1.40
10???????4???????????2.25????????0.11???????????1.69
11???????5???????????2.98????????0.10???????????1.90
12???????6???????????2.90????????0.08???????????2.17
Embodiment 8
The 10.0g Rosmarinus officinalis leaf of packing in the circulation extractor is pulverized material (particle is less than 2mm), puts into 50～150mL polar solvent (as 95% ethanol) in the susceptor of bottom, and 3～4h is extracted in circulation, cooling; With the extracting solution normal pressure or the underpressure distillation of polar solvent, obtain brown or blackish green medicinal extract (being general extractive); Medicinal extract is reinstalled in the extractor, nonpolar or the weak polar solvent with 50mL is (as 30～60 ℃ of sherwood oils, 60～90 ℃ of sherwood oils, normal hexane, chloroform, ether, methylene dichloride, 1, the 2-ethylene dichloride) carries out extract at low temperature, extracting solution obtains dark half liquid half material admittedly through underpressure distillation again, obtains colourless or light yellow rosemary ethereal oil through steam distillation again; The rosemary antioxidant crude product that medicinal extract obtains after nonpolar or weak polar solvent extracting (the results are shown in Table 3).
Rosemary ethereal oil and rosemary antioxidant comprehensively extract the result under different non-(weak) polar solvent conditions of table 3
No non-(weak) polar solvent general extractive (g) essential oil (g) rosemary antioxidant crude product (g)
13 30～60 ℃ of sherwood oils 1.79 0.12 1.69
14 60～90 ℃ of sherwood oils 1.79 0.13 1.57
15 normal hexanes-chloroform (1: 1) 1.79 0.14 0.98
16 chloroforms 1.79 0.16 0.78
17 normal hexanes 1.79 0.10 1.50
18 ether 1.79 0.08 1.18
19 methylene dichloride 1.79 0.12 1.26
20 1,2-ethylene dichloride 1.79 0.08 1.06
Embodiment 9
36.0～72.0g Rosmarinus officinalis leaf of packing in the circulation extractor (contains essential oil or does not contain essential oil, do not pulverize), add sherwood oil mixed solution (as sherwood oil, sherwood oil-ethanol, sherwood oil-alcohol-water, petroleum ether-ethyl acetate, sherwood oil-ethanol-ethyl acetate, petroleum ether-ethyl acetate-water, the sherwood oil-water etc.) 150～400mL that contains the segment polarity solvent, 3～4h is extracted in the reflux circulation, cooling; From extract collector, directly obtain light solid and dark extracting solution, filtration, a little petroleum ether, obtain light yellow or oyster rosemary antioxidant (the results are shown in Table 4), dark extracting solution normal pressure or underpressure distillation can also the recovery part antioxidants.Use contains the rosemary leave period of the day from 11 p.m. to 1 a.m of essential oil, can obtain a small amount of rosemary ethereal oil from the extracting solution of removing solvent.
Table 4 contains the sherwood oil mixed solution one step extraction rosemary antioxidant result of segment polarity solvent
No Rosmarinus officinalis leaf (g) sherwood oil mixed solution light color rosemary antioxidant (g)
21 72.0 sherwood oils 0.8
22 30.0 sherwood oils-water (90: 10) 0.3
23 36.0 sherwood oils-ethanol (95: 5) 3.0
24 36.0 sherwood oils-alcohol-water (90: 7.5: 2.5) 3.0
25 36.0 sherwood oils-alcohol-water (80: 15: 5) 5.5
26 50.7 sherwood oils-alcohol-water (94: 5: 1) 4.3
27 30.0 petroleum ether-ethyl acetates (90: 10) 0.8
28 30.0 sherwood oils-ethanol-ethyl acetate (90: 7: 3) 3.6
Embodiment 10
The 50.0g Rosmarinus officinalis leaf of packing in the circulation extractor (contains essential oil or does not contain essential oil, do not pulverize), adding 300～400mL ethanol (or 95% ethanol etc.), and load ultrasonic wave (groove type ultrasonic wave producer or probe type ultrasonic wave producer) respectively, strengthen this circulation leaching process, under room temperature or natural soaking condition, extract 10～30min, filter and concentrate, and after nonpolar or weak polar solvent extracting, obtain colourless or light yellow rosemary ethereal oil and rosemary antioxidant crude product (the results are shown in Table 5) respectively.
Rosemary antioxidant comprehensively extracts the result under the different ultrasonic wave conditions of table 5
| No | Ultrasonic wave | Rosemary antioxidant product (g) | |||
| Mode | Frequency (KHz) | Power (W) | Extraction time (min) | ||
| 29 30 | The slot type sonde-type | ??33 ??20～25 | ??250 ??1000 | ??30 ??10 | ??6.40 ??6.70 |
Embodiment 11
Other steps that circulation is extracted with 6.0g rosemary antioxidant product, add aqueous ethanolic solution and the 0.6～1.5g gac of 30～120mL 50～95% with embodiment 6, in 50～100 ℃ of stirred in water bath 15～30min, filter; The filtrate concentrate under reduced pressure at low temperature is used 30～120mL distilled water diluting again, and filtration drying obtains light yellow or light salmon rosemary antioxidant 4.6g.
Claims (7)
1. the combined extraction method of rosemary ethereal oil and rosemary antioxidant, it is characterized in that extracting rosemary leave material 0.08～6h 20～100 ℃ of direct down circulations with the polar organic solvent of 3～20 times of weight that are equivalent to the rosemary leave material, acquisition is dissolved in the rosemary ethereal oil of polar organic solvent and the solution of rosemary antioxidant, nonpolar or weakly polar organic solvent with 3～200 times of weight of mixture that are equivalent to rosemary ethereal oil and rosemary antioxidant extracts rosemary ethereal oil and rosemary antioxidant 0.08～6h 20～100 ℃ of direct down circulations, and be cooled to 5～30 ℃, acquisition is dissolved in the rosemary ethereal oil of nonpolar or weakly polar organic solvent and the rosemary antioxidant of precipitation shape, filter, obtain the throw out rosemary antioxidant, extracting solution boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
2. the combined extraction method of rosemary ethereal oil according to claim 1 and rosemary antioxidant is characterized in that comprising following two steps:
The first step: use the polar organic solvent that is equivalent to 3～20 times of weight of rosemary leave material directly to circulate down at 20～100 ℃ and extract rosemary leave material 0.08～6h, extracting solution is boiled off solvent under 20～100 ℃, obtain the mixture of rosemary ethereal oil and rosemary antioxidant;
Second step: at 20～100 ℃ of nonpolar or weakly polar organic solvents of using 3～20 times of weight of mixture that are equivalent to above-mentioned rosemary ethereal oil and rosemary antioxidant down, directly the mixture 0.5～6h of above-mentioned rosemary ethereal oil and rosemary antioxidant is extracted in circulation, be cooled to 5～30 ℃, filter, the solid that obtains is the rosemary antioxidant product, filtrate boils off solvent under 20～100 ℃, obtain the rosemary ethereal oil product.
3. the combined extraction method of rosemary ethereal oil according to claim 1 and rosemary antioxidant, it is characterized in that: under 20～100 ℃, mixed organic solvents with polar organic solvent and nonpolar or weakly polar organic solvent, directly rosemary leave material 0.08～6h is extracted in circulation, the gross weight of the mixed organic solvents of wherein nonpolar or weakly polar organic solvent and polar organic solvent is 3～20 times of rosemary leave material weight, it is 0.1～20% that the weight of polar organic solvent accounts for per-cent nonpolar or weakly polar organic solvent and polar organic solvent gross weight, postcooling to 5～30 ℃ are extracted in circulation, obtain containing the extracting solution of light insoluble solids rosemary antioxidant, filter, the solid that obtains is the rosemary antioxidant product, and filtrate boils off solvent and obtains the rosemary ethereal oil product under 20～100 ℃.
4. according to the combined extraction method of claim 1 or 2 or 3 described rosemary ethereal oils and rosemary antioxidant, it is characterized in that: rosemary leave material circulation leaching process can adopt ultrasonic wave to strengthen the effect of extraction synchronously, ultrasonic frequency 20～40KHz, ultrasonic power 100～2000W, circulation extraction time 5～60min.
5. according to the combined extraction method of claim 2 or 3 described rosemary ethereal oils and rosemary antioxidant, it is characterized in that and the rosemary antioxidant product can be purified, method is as follows: add 50～95% the aqueous ethanolic solution of 5～20 times of weight and the gac of 0.10～0.25 times of weight, in 50～100 ℃ of water-baths, stir 15～30min, filter; The filtrate concentrate under reduced pressure at low temperature is used 30～120mL distilled water diluting again, filters, and drying obtains light solid rosemary antioxidant.
6. the combined extraction method of rosemary ethereal oil according to claim 1 and rosemary antioxidant is characterized in that polar solvent is 95% ethanol.
7. the combined extraction method of rosemary ethereal oil according to claim 1 and rosemary antioxidant is characterized in that nonpolar or weakly polar organic solvent is a sherwood oil, and it is 20～100 ℃ that temperature is extracted in circulation.
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Cited By (7)
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| CN102031116A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学科教开发部 | New method for preparing rosemary natural antioxidant |
| CN101658489B (en) * | 2008-08-27 | 2011-11-23 | 海南四环心脑血管药物研究院有限公司 | Nalmefene hydrochloride injection and preparation method thereof |
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| CN1076380C (en) * | 1995-01-13 | 2001-12-19 | 金坚敏 | Efficient natural antioxidants and their preparation |
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| CN113372997A (en) * | 2021-06-17 | 2021-09-10 | 福建省农业科学院亚热带农业研究所（福建省农业科学院蔗麻研究中心） | Method for carrying out segmented temperature control extraction on main components of rosemary |
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